阅读说明：本技术 一种电子俘获检测器以及气相装置 (electron capture detector and gas phase device ) 是由 刘召贵 张轩 吴明所 周立 于 2019-10-21 设计创作，主要内容包括：本发明公开了一种电子俘获检测器以及气相装置,其特征在于,检测器包括阳极封装件、阴极组件、放射源以及加热组件,阴极组件具有中心通孔,阴极的顶部通过绝缘套套设在阳极封装件的外部,底部设有用于与色谱柱相连接的连接结构,从而在绝缘套、阴极组件内壁、连接结构之间形成一个垂直腔体,垂直腔体的底部侧壁设置有放射源,阴极组件的侧壁设置有与垂直腔体相连通的出气通道,连接结构的侧壁设置有与中心通孔相连通的尾吹气通道；本发明的阳极封装件由阳极和绝缘件封装为一个整体,由于绝缘件与中心通孔间隙配合,能够保证阳极在安装过程中不相对于中心通孔发生偏向,且装配简单,无需特殊的装配工具。(The invention discloses an electron capture detector and a gas phase device, which are characterized in that the detector comprises an anode packaging part, a cathode component, a radioactive source and a heating component, wherein the cathode component is provided with a central through hole, the top of a cathode is sleeved outside the anode packaging part through an insulating sleeve, the bottom of the cathode is provided with a connecting structure used for being connected with a chromatographic column, so that a vertical cavity is formed among the insulating sleeve, the inner wall of the cathode component and the connecting structure, the side wall of the bottom of the vertical cavity is provided with the radioactive source, the side wall of the cathode component is provided with a gas outlet channel communicated with the vertical cavity, and the side wall of the connecting structure is provided with a tail gas blowing; the anode packaging part is formed by packaging the anode and the insulating part into a whole, and the insulating part is in clearance fit with the central through hole, so that the anode is prevented from deviating relative to the central through hole in the installation process, the assembly is simple, and a special assembly tool is not needed.)

1. An electron capture detector comprising an anode package, a cathode assembly, a radiation source, and a heating assembly;

The cathode assembly is provided with a central through hole, the top of the cathode is sleeved outside the anode packaging part through an insulating sleeve, the bottom of the cathode is provided with a connecting structure used for being connected with a chromatographic column, so that a vertical cavity is formed among the insulating sleeve, the inner wall of the cathode assembly and the connecting structure, the side wall of the bottom of the vertical cavity is provided with a radioactive source, the side wall of the cathode assembly is provided with an air outlet channel communicated with the vertical cavity, and the side wall of the connecting structure is provided with a tail air blowing channel communicated with the central through hole; the heating component is abutted against the cathode component and is provided with a heating structure for providing heat for the vertical cavity.

2. An electron capture detector according to claim 1, wherein the anode package comprises an anode and an insulator packaged outside the anode, and the top of the cathode assembly is sleeved outside the anode by the insulator sleeve.

3. An electron capture detector according to claim 2 wherein the inner wall of the cathode assembly is in clearance fit with the insulator.

4. An electron capture detector according to claim 2, wherein the insulator is an insulator of thermally insulating material.

5. The electron capture detector of claim 1, wherein the heating assembly comprises a heat conducting block abutting the cathode assembly and configured to provide heat to the vertical cavity, a heating element disposed within the heat conducting block and configured to generate heat, and a temperature feedback element configured to monitor temperature in real time.

6. An electron capture detector according to claim 1, wherein the connecting structure is a guide sleeve structure of a chromatography column.

7. The electron capture detector of claim 1, wherein said cathode assembly comprises a cathode, an ionization chamber weld disposed at a lower end of said cathode, an ionization chamber end cap disposed within said ionization chamber weld, and said attachment structure removably disposed at a lower end of said ionization chamber weld;

The inner wall of the ionization chamber welding piece is provided with a positioning concave surface, the positioning concave surface and the air outlet channel are oppositely arranged, the side surface of the ionization chamber end cover is provided with a fixed angle direction structure matched with the positioning concave surface and an air outlet hole communicated with the end cover center through hole, and the fixed angle direction structure and the air outlet hole are oppositely arranged, so that the ionization chamber end cover is ensured to be communicated with the air outlet channel after being installed on the inner wall of the ionization chamber welding piece.

8. An electron capture detector according to claim 7 wherein a metal sealing gasket is provided between the cathode and the ionization chamber weldment.

9. An electron capture detector according to claim 1, wherein the detector further comprises an electron flow controller comprising a carrier gas controller and a tail gas controller;

The radioactive source is a sleeve-shaped structure made by rolling a nickel sheet plated with ⁶³ Ni, and the sleeve-shaped structure is assembled on the side wall of the bottom of the vertical cavity.

10. A gas phase apparatus comprising an electron capture detector according to any one of claims 1 to 9.

Technical Field

The invention relates to the technical field of gas chromatographs, in particular to an electron capture detector and a gas phase device.

Background

an Electron Capture Detector (ECD) is a common Detector in gas chromatography, and is a gas chromatography Detector with high sensitivity and an earliest selectivity Detector; it only responds to compounds capable of capturing electrons, such as halogenated hydrocarbons and compounds containing heteroatoms such as N, O and S, and has been widely used for analyzing trace pesticides, polychlorinated biphenyl and the like in environmental samples for many years due to high sensitivity and good selectivity.

Disclosure of Invention

In view of the above, there is a need to overcome at least one of the above-mentioned defects in the prior art, and the present invention provides an electron capture detector, including an anode package, a cathode assembly, a radiation source and a heating assembly, wherein the cathode assembly has a central through hole, the top of the cathode assembly is sleeved outside the anode package through an insulating sleeve, the bottom of the cathode assembly is provided with a connecting structure for connecting with a chromatographic column, so as to form a vertical cavity between the insulating sleeve, the inner wall of the cathode assembly and the connecting structure, the bottom side wall of the vertical cavity is provided with the radiation source, the side wall of the cathode assembly is provided with an air outlet channel communicated with the vertical cavity, and the side wall of the connecting structure is provided with a tail air blowing channel communicated with the central through hole; the heating component is abutted against the cathode component and is provided with a heating structure for providing heat for the vertical cavity.

According to the prior art in the background of the patent, when the conventional electron capture detector is installed, the coaxiality of the central through hole of the anode and the central through hole of the cathode needs to be ensured, namely the anode and the cathode are insulated, so that the requirements on machining and assembling technology are high, the anode and the cathode need to work in a high-temperature environment, and the insulating guide sleeve has instability in a long-term high-temperature environment; meanwhile, the insulating part meets the insulating requirement; moreover, the insulating part has certain thickness, can play the effect of keeping apart high temperature to can reduce the influence of high temperature to insulating cover.

In addition, the electron capture detector disclosed by the invention also has the following additional technical characteristics:

Further, the anode packaging part comprises an anode and an insulating part packaged outside the anode, and the top of the cathode assembly is sleeved outside the anode through the insulating sleeve.

Further, the inner wall of the cathode assembly is in clearance fit with the insulator.

Further, the insulator is made of a heat insulating material.

Further, the insulating part is an insulating cylinder made of ceramic, and the anode is a metal anode.

Further, the heating assembly comprises a heat conduction block which is abutted with the cathode assembly and used for providing heat for the vertical cavity, a heating element which is arranged in the heat conduction block and used for generating heat, and a temperature feedback element which is used for monitoring the temperature in real time.

Furthermore, the connecting structure is a chromatographic column guide shaft sleeve structure and is used for connecting a chromatographic column.

Further, the cathode assembly comprises a cathode, an ionization chamber welding piece detachably arranged at the lower end part of the cathode, an ionization chamber end cover arranged in the ionization chamber welding piece, and the connecting structure fixedly arranged at the lower end part of the ionization chamber welding piece through a clamping sleeve nut, so that an ionization chamber cavity is formed between the lower end part of the ionization chamber end cover and the bottom of the radioactive source in the ionization chamber welding piece.

Furthermore, the cathode and the ionization chamber welding part are respectively provided with a corresponding cathode through hole and an ionization chamber through hole, and the cathode through hole and the ionization chamber through hole form the central through hole.

furthermore, the outer wall of the top of the cathode is provided with an external thread, the inner wall of the top of the cathode is sleeved outside the anode through the insulating sleeve and is connected with the external thread of the top of the cathode through a locking nut so as to be fixedly connected with the anode, and the bottom of the cathode is fixedly connected with the ionization chamber welding piece through a thread.

Furthermore, an ionization chamber end cover is arranged in the ionization chamber through hole, is positioned between the insulating piece and the radioactive source and is provided with an end cover central through hole into which the anode extends.

Further, an internal thread is arranged in the central through hole of the end cover.

When the ionization chamber end cover is installed, the internal thread is arranged in the central through hole of the end cover, so that the screw rod with the external thread matched with the internal thread can be screwed into the central through hole of the end cover, and the ionization chamber end cover can be fed into the through hole of the ionization chamber through the screw rod and then screwed out of the screw rod; when the radioactive source is taken out of the ionization chamber welding part, the ionization chamber end cover needs to be taken out firstly, when the ionization chamber end cover is taken out, the screw is screwed into the internal thread, and then the ionization chamber end cover is pulled out by pulling out the screw, so that the ionization chamber end cover is convenient to take and install, and the installation and the replacement of the radioactive source positioned at the lower part of the ionization chamber end cover are simpler and more convenient.

Furthermore, a positioning concave surface is arranged on the inner wall of the ionization chamber welding piece and is opposite to the air outlet channel, a fixed-angle-direction structure matched with the positioning concave surface and an air outlet hole communicated with the end cover center through hole are arranged on the side surface of the ionization chamber end cover, and the fixed-angle-direction structure and the air outlet hole are opposite to each other, so that the ionization chamber end cover is ensured to be communicated with the air outlet channel after being installed on the inner wall of the ionization chamber welding piece. Further, a metal sealing gasket is arranged between the cathode and the ionization chamber welding piece.

Furthermore, the detector also comprises a mounting plate and a shell arranged on the mounting plate, wherein the top inner wall of the shell is positioned above the top of the cathode; the part of the ionization chamber welding piece above the radioactive source is fixed on the mounting plate through a fastener.

Further, the heat conduction block is fixed on the mounting plate by a fastener.

Furthermore, the detector also comprises a heat preservation shell arranged on the mounting plate through a fastener, and the top of the heat preservation shell is provided with a cathode extending hole for extending the top of the cathode.

Furthermore, the heat preservation shell is filled with heat preservation materials.

Further, the detector also comprises an electronic flow controller, and the electronic flow controller comprises a carrier gas controller and a tail gas blowing controller.

furthermore, the radioactive source is a sleeve-shaped structure made of rolled nickel sheets plated with ⁶³ Ni, and the sleeve-shaped structure is assembled on the side wall of the bottom of the vertical cavity.

According to another aspect of the present invention, there is also provided a gas phase apparatus, characterized by comprising the above-described electron capture detector.

Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.

Drawings

The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:

FIG. 1 is a schematic diagram of an electron capture detector according to the present invention; and

FIG. 2 is a schematic structural diagram of an anode package according to the present invention; and

FIG. 3 is a cross-sectional view of the electron capture detector of the present invention taken along line A-A of FIG. 1.

The device comprises a locking nut 1, an insulating sleeve 2, a shell 3, a heat preservation shell 4, a cathode 5, a metal sealing gasket 6, an anode packaging part 7, an anode 71, an insulating part 72, an ionization chamber end cover 8, a positioning angle structure 81, an air outlet 82, an ionization chamber welding part 9, a positioning concave surface 91, a mounting plate 10, a radioactive source 11, a heating assembly 12, a ferrule nut 13 and a connecting structure 14.

Detailed Description

Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout; the embodiments described below with reference to the drawings are illustrative only and should not be construed as limiting the invention.

In the description of the present invention, it is to be understood that the terms "upper", "lower", "bottom", "top", "front", "rear", "inner", "outer", "lateral", "vertical", and the like, indicate orientations and positional relationships based on the orientations and positional relationships shown in the drawings, are used only for convenience in describing the present invention and for simplification of description, and do not indicate or imply that the device or element being referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention.

The conception of the invention is that the anode packaging part is packaged into a whole by the anode and the insulating part, and in the installation process of the anode, because the insulating part is in clearance fit with the central through hole, the anode can be ensured not to deflect relative to the central through hole in the installation process, thereby ensuring the coaxiality of the anode and the ionization chamber cavity, and the invention has simple assembly and does not need special assembly tools; moreover, the insulating part has certain thickness, can play the effect of keeping apart high temperature to can reduce the influence of high temperature to insulating cover.

FIG. 1 is a schematic diagram of an electron capture detector according to the present invention; FIG. 2 is a schematic structural diagram of an anode package according to the present invention; and FIG. 3 is a cross-sectional view of the electron capture detector of the present invention taken along line A-A of FIG. 1.

As shown in fig. 1-3, according to an embodiment of the present invention, an electron capture detector includes an anode package 7, a cathode assembly, a radiation source 11 and a heating assembly 12, the cathode assembly is provided with a central through hole, the top of the cathode assembly is sleeved outside the anode packaging part 7 through an insulating sleeve 2, the bottom of the cathode assembly is provided with a connecting structure 14 used for being connected with a chromatographic column (used for flowing carrier gas G1 in the chromatographic column), so as to form a vertical cavity between the insulating sleeve 2, the inner wall of the cathode assembly and the connecting structure 14, the side wall of the bottom of the vertical cavity is provided with a radioactive source 11, the side wall of the cathode assembly is provided with an air outlet channel communicated with the vertical cavity and used for allowing waste gas G3 to flow out, the side wall of the connecting structure 14 is provided with a tail blowing channel which is communicated with the central through hole and is used for leading tail blowing air to flow into G2; the heating component 12 is abutted against the cathode component and is provided with a heating structure for providing heat to the vertical cavity.

According to the prior art in the background of the patent, when the conventional electron capture detector is installed, the coaxiality of an anode 71 and a central through hole of the cathode needs to be ensured, namely the insulation between the cathode and the anode is ensured, so that the machining requirement and the assembly technical requirement are high, moreover, the anode 71 and the cathode 5 need to work in a high-temperature environment, and an insulation guide sleeve has instability in a long-term high-temperature environment; meanwhile, the insulation member 72 meets the insulation requirements; furthermore, the insulating member 72 has a certain thickness, which can isolate high temperature, thereby reducing the influence of high temperature on the insulating sleeve 2.

In addition, the electron capture detector disclosed by the invention also has the following additional technical characteristics:

According to some embodiments of the present invention, the anode package 7 comprises an anode 71 and an insulating member 72 packaged outside the anode 71, and the top of the cathode assembly is sleeved outside the anode 71 through the insulating sleeve 2, as shown in fig. 1 and 2.

According to some embodiments of the invention, the inside wall of the cathode assembly is clearance fit with the insulator 72, as shown in fig. 1 and 2.

According to some embodiments of the present invention, the insulator 72 is an insulator 72 made of a heat insulating material.

According to some embodiments of the invention, the insulator 72 is an insulating cylinder made of ceramic and the anode 71 is a metal anode.

According to some embodiments of the invention, the heating assembly 12 includes a heat conducting block abutting the cathode assembly and for providing heat to the vertical cavity, and a heating element disposed within the heat conducting block for generating heat and a temperature feedback element for monitoring temperature in real time.

According to some embodiments of the present invention, the connecting structure 14 is a column guide sleeve structure for connecting a chromatography column, as shown in FIG. 1.

According to some embodiments of the present invention, the cathode assembly comprises a cathode 5, an ionization chamber welding piece 9 detachably disposed at the lower end of the cathode 5, an ionization chamber end cap 8 disposed in the ionization chamber welding piece 9, and the connecting structure 14 fixedly disposed at the lower end of the ionization chamber welding piece 9 through a ferrule nut 13, as shown in fig. 1, so that an ionization chamber is formed in the ionization chamber welding piece 9 between the lower end of the ionization chamber end cap 8 and the bottom of the radiation source 11.

According to some embodiments of the invention, the cathode 5 and the ionization chamber weldment 9 have corresponding cathode through holes and ionization chamber through holes, respectively, which constitute the central through hole, as shown in fig. 1.

According to some embodiments of the present invention, the outer wall of the top of the cathode 5 is provided with an external thread, the inner wall of the top of the cathode 5 is sleeved outside the anode 71 through the insulating sleeve 2 and is connected with the external thread of the top of the cathode 5 through the locking nut 1 so as to be fixedly connected with the anode 71, and the bottom of the cathode 5 is connected with the ionization chamber welding part 9 through a thread, as shown in fig. 1.

According to some embodiments of the present invention, an ionization chamber end cap 8 is disposed in the ionization chamber through hole, and the ionization chamber end cap 8 is located between the insulator 72 and the radiation source 11 and has an end cap central through hole into which the anode 71 extends, as shown in fig. 1.

According to one embodiment of the invention, the end cap central through hole is internally threaded.

When the ionization chamber end cover 8 is installed, the internal thread is arranged in the central through hole of the end cover, so that the screw rod with the external thread matched with the internal thread can be screwed into the central through hole of the end cover, and the ionization chamber end cover 8 can be fed into the through hole of the ionization chamber and then screwed out of the screw rod through the screw rod; when the radioactive source 11 is taken out of the ionization chamber welding part, the ionization chamber end cover 8 needs to be taken out firstly, when the ionization chamber end cover 8 is taken out, the screw is screwed into the internal thread, and then the ionization chamber end cover 8 is pulled out by pulling out the screw, so that the ionization chamber end cover 8 is convenient to take and install, and the installation and the replacement of the radioactive source 11 positioned at the lower part of the ionization chamber end cover 8 are simpler and more convenient.

Furthermore, a positioning concave surface 91 is arranged on the inner wall of the ionization chamber welding part 9, the positioning concave surface 91 and the air outlet channel are arranged in an opposite mode, the side surface of the ionization chamber end cover 8 is provided with a fixed angle structure 81 matched with the positioning concave surface and an air outlet 82 communicated with the end cover center through hole, the fixed angle structure 81 and the air outlet 82 are arranged in an opposite mode, and therefore the ionization chamber end cover 8 is guaranteed to be communicated with the air outlet channel after being installed on the inner wall of the ionization chamber welding part 9, as shown in fig. 1 and 3.

According to some embodiments of the invention, a metal sealing gasket 6 is provided between the cathode 5 and the ionization chamber weldment 9, as shown in fig. 1.

According to some embodiments of the invention, the detector further comprises a mounting plate 10 and a housing 3 disposed on the mounting plate 10, a top inner wall of the housing 3 being located above a top of the cathode 5; the portion of the ionization chamber weldment 9 above the radiation source 11 is secured to the mounting plate 10 by fasteners, as shown in fig. 1.

according to some embodiments of the present invention, the heat conducting block is fixed to the mounting plate 10 by fasteners, as shown in fig. 1.

According to some embodiments of the present invention, the detector further comprises an insulating case 4 disposed on the mounting plate 10 by a fastener, and a top portion of the insulating case 4 has a cathode extension hole through which a top portion of the cathode 5 extends, as shown in fig. 1.

According to some embodiments of the invention, the insulating shell 4 is filled with an insulating material.

According to some embodiments of the invention, the detector further comprises an electronic flow controller comprising a carrier gas controller and a tail gas controller.

According to some embodiments of the invention, the radiation source is a sleeve-like structure made of rolled nickel sheets plated with ⁶³ Ni, which is fitted on the bottom side wall of the vertical cavity.

According to another aspect of the present invention, there is also provided a gas phase apparatus, characterized by comprising the above-described electron capture detector.

Any reference to "one embodiment," "an embodiment," "example embodiment," etc., means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment of the invention; the schematic representations in various places in the specification do not necessarily refer to the same embodiment; further, when a particular feature, structure, or characteristic is described in connection with any embodiment, it is submitted that it is within the purview of one skilled in the art to effect such feature, structure, or characteristic in connection with other ones of the embodiments.

While specific embodiments of the invention have been described in detail with reference to a number of illustrative embodiments thereof, it should be understood that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the spirit and scope of the principles of this invention; in particular, reasonable variations and modifications are possible in the component parts and/or arrangements of the subject combination arrangement within the scope of the foregoing disclosure, the drawings and the appended claims without departing from the spirit of the invention; except variations and modifications in the component parts and/or arrangements, the scope of which is defined by the appended claims and equivalents thereof.